#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/28/4312815.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4312815
loop_
_publ_author_name
'Karl M. Kadish'
'Tuan D. Phan'
'Lingamallu Giribabu'
'Eric Van Caemelbecke'
'John L. Bear'
_publ_section_title
;
 Substituent and Isomer Effects on Structural, Spectroscopic, and
 Electrochemical Properties of Dirhodium(III,II) Complexes Containing Four
 Identical Unsymmetrical Bridging Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8663
_journal_page_last               8673
_journal_paper_doi               10.1021/ic034963l
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         'C44 H32 N8 F4 Cl Rh2, 2 C H2 Cl2'
_chemical_formula_sum            'C46 H36 Cl5 F4 N8 Rh2'
_chemical_formula_weight         1159.90
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           104
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4 -2n'
_symmetry_space_group_name_H-M   'P 4 n c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.2139(8)
_cell_length_b                   15.2139(8)
_cell_length_c                   9.6116(7)
_cell_measurement_reflns_used    4116
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      23.24
_cell_measurement_theta_min      1.89
_cell_volume                     2224.7(2)
_computing_cell_refinement       'Bruker SAINT software (Bruker, 1999)'
_computing_data_collection       'Siemens SMART software (Siemens, 1996)'
_computing_data_reduction        'Bruker SAINT software (Bruker, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      223(2)
_diffrn_detector_area_resol_mean 1K
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_av_sigmaI/netI    0.0239
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            6685
_diffrn_reflns_theta_full        23.24
_diffrn_reflns_theta_max         23.24
_diffrn_reflns_theta_min         1.89
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    1.104
_exptl_absorpt_correction_T_max  0.9187
_exptl_absorpt_correction_T_min  0.7386
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.731
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Square column'
_exptl_crystal_F_000             1158
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.362
_refine_diff_density_min         -0.203
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.04(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     150
_refine_ls_number_reflns         1490
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0207
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0179P)²+2.3347P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0480
_refine_ls_wR_factor_ref         0.0541
_reflns_number_gt                1230
_reflns_number_total             1672
_reflns_threshold_expression     >4igma(I)
_cod_data_source_file            ic034963lsi20030917_093709.cif
_cod_data_source_block           k677
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_formula_sum        'C46 H36 N8 F4 Cl5 Rh2'
_cod_database_code               4312815
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.5000 0.5000 0.52043(9) 0.01986(18) Uani 1 4 d S . .
Rh2 Rh 0.5000 0.5000 0.77144(4) 0.01807(19) Uani 1 4 d S . .
Cl1 Cl 0.5000 0.5000 0.2675(3) 0.0309(5) Uani 1 4 d S . .
Cl2 Cl 0.46085(10) 0.08724(10) 0.3729(2) 0.0679(4) Uani 1 1 d . . .
F1 F 0.58798(19) 0.23358(18) 0.7196(3) 0.0497(8) Uani 1 1 d . . .
N1 N 0.4235(2) 0.3883(2) 0.5331(4) 0.0218(8) Uani 1 1 d . . .
N2 N 0.4703(2) 0.3716(2) 0.7615(4) 0.0209(7) Uani 1 1 d . . .
C1 C 0.3715(3) 0.3623(3) 0.4264(5) 0.0304(10) Uani 1 1 d . . .
H1 H 0.3661 0.3995 0.3488 0.036 Uiso 1 1 calc R . .
C2 C 0.3266(3) 0.2851(3) 0.4263(5) 0.0356(12) Uani 1 1 d . . .
H2 H 0.2906 0.2696 0.3507 0.043 Uiso 1 1 calc R . .
C3 C 0.3350(3) 0.2290(3) 0.5410(5) 0.0379(11) Uani 1 1 d . . .
H3 H 0.3062 0.1743 0.5425 0.045 Uiso 1 1 calc R . .
C4 C 0.3853(3) 0.2546(2) 0.6493(6) 0.0315(9) Uani 1 1 d . . .
H4 H 0.3917 0.2168 0.7260 0.038 Uiso 1 1 calc R . .
C5 C 0.4288(2) 0.3373(2) 0.6500(6) 0.0242(8) Uani 1 1 d . . .
C6 C 0.4974(2) 0.3154(3) 0.8721(5) 0.0225(10) Uani 1 1 d . . .
C7 C 0.5598(3) 0.2500(3) 0.8506(5) 0.0322(11) Uani 1 1 d . . .
C8 C 0.5937(3) 0.2003(3) 0.9588(6) 0.0422(14) Uani 1 1 d . . .
H8 H 0.6358 0.1564 0.9415 0.051 Uiso 1 1 calc R . .
C9 C 0.5648(3) 0.2163(3) 1.0919(5) 0.0416(13) Uani 1 1 d . . .
H9 H 0.5878 0.1838 1.1667 0.050 Uiso 1 1 calc R . .
C10 C 0.5026(3) 0.2796(3) 1.1159(5) 0.0382(13) Uani 1 1 d . . .
H10 H 0.4823 0.2896 1.2069 0.046 Uiso 1 1 calc R . .
C11 C 0.4695(3) 0.3286(3) 1.0071(5) 0.0293(10) Uani 1 1 d . . .
H11 H 0.4270 0.3720 1.0253 0.035 Uiso 1 1 calc R . .
C12 C 0.5000 0.0000 0.2720(14) 0.072(2) Uani 1 2 d S . .
H12 H 0.5465 0.0209 0.2144 0.086 Uiso 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Rh1 N1 89.799(14) . 3_655 ?
N1 Rh1 N1 173.2(2) . 2_665 ?
N1 Rh1 N1 89.799(14) 3_655 2_665 ?
N1 Rh1 N1 89.799(14) . 4_565 ?
N1 Rh1 N1 173.2(2) 3_655 4_565 ?
N1 Rh1 N1 89.799(14) 2_665 4_565 ?
N1 Rh1 Rh2 86.60(11) . . ?
N1 Rh1 Rh2 86.60(11) 3_655 . ?
N1 Rh1 Rh2 86.60(11) 2_665 . ?
N1 Rh1 Rh2 86.60(11) 4_565 . ?
N1 Rh1 Cl1 93.40(11) . . ?
N1 Rh1 Cl1 93.40(11) 3_655 . ?
N1 Rh1 Cl1 93.40(11) 2_665 . ?
N1 Rh1 Cl1 93.40(11) 4_565 . ?
Rh2 Rh1 Cl1 180.000(1) . . ?
N2 Rh2 N2 89.871(12) 2_665 3_655 ?
N2 Rh2 N2 174.6(2) 2_665 . ?
N2 Rh2 N2 89.871(11) 3_655 . ?
N2 Rh2 N2 89.871(11) 2_665 4_565 ?
N2 Rh2 N2 174.6(2) 3_655 4_565 ?
N2 Rh2 N2 89.871(12) . 4_565 ?
N2 Rh2 Rh1 87.28(11) 2_665 . ?
N2 Rh2 Rh1 87.28(11) 3_655 . ?
N2 Rh2 Rh1 87.28(11) . . ?
N2 Rh2 Rh1 87.28(11) 4_565 . ?
C1 N1 C5 119.4(4) . . ?
C1 N1 Rh1 121.7(3) . . ?
C5 N1 Rh1 118.9(3) . . ?
C5 N2 C6 119.7(3) . . ?
C5 N2 Rh2 121.3(3) . . ?
C6 N2 Rh2 118.9(3) . . ?
N1 C1 C2 123.1(5) . . ?
C1 C2 C3 118.7(4) . . ?
C4 C3 C2 118.9(4) . . ?
C3 C4 C5 121.5(5) . . ?
N2 C5 N1 117.4(3) . . ?
N2 C5 C4 124.4(5) . . ?
N1 C5 C4 118.1(5) . . ?
C11 C6 C7 117.0(4) . . ?
C11 C6 N2 121.7(4) . . ?
C7 C6 N2 121.0(4) . . ?
F1 C7 C8 118.7(4) . . ?
F1 C7 C6 119.1(4) . . ?
C8 C7 C6 122.2(5) . . ?
C9 C8 C7 118.9(5) . . ?
C10 C9 C8 120.2(5) . . ?
C9 C10 C11 120.3(5) . . ?
C10 C11 C6 121.5(4) . . ?
Cl2 C12 Cl2 112.6(7) . 2_655 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 N1 2.063(3) . ?
Rh1 N1 2.063(3) 3_655 ?
Rh1 N1 2.063(3) 2_665 ?
Rh1 N1 2.063(3) 4_565 ?
Rh1 Rh2 2.4127(9) . ?
Rh1 Cl1 2.431(3) . ?
Rh2 N2 2.007(3) 2_665 ?
Rh2 N2 2.007(3) 3_655 ?
Rh2 N2 2.007(3) . ?
Rh2 N2 2.007(3) 4_565 ?
Cl2 C12 1.748(7) . ?
F1 C7 1.353(5) . ?
N1 C1 1.355(6) . ?
N1 C5 1.367(6) . ?
N2 C5 1.349(6) . ?
N2 C6 1.425(6) . ?
C1 C2 1.360(6) . ?
C2 C3 1.400(7) . ?
C3 C4 1.349(7) . ?
C4 C5 1.423(5) . ?
C6 C11 1.379(6) . ?
C6 C7 1.392(6) . ?
C7 C8 1.385(6) . ?
C8 C9 1.375(7) . ?
C9 C10 1.370(7) . ?
C10 C11 1.380(6) . ?
C12 Cl2 1.748(7) 2_655 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Rh1 Rh2 N2 -158.61(11) . . . 2_665 ?
N1 Rh1 Rh2 N2 111.39(11) 3_655 . . 2_665 ?
N1 Rh1 Rh2 N2 21.39(11) 2_665 . . 2_665 ?
N1 Rh1 Rh2 N2 -68.61(11) 4_565 . . 2_665 ?
Cl1 Rh1 Rh2 N2 32(100) . . . 2_665 ?
N1 Rh1 Rh2 N2 111.39(11) . . . 3_655 ?
N1 Rh1 Rh2 N2 21.39(11) 3_655 . . 3_655 ?
N1 Rh1 Rh2 N2 -68.61(11) 2_665 . . 3_655 ?
N1 Rh1 Rh2 N2 -158.61(11) 4_565 . . 3_655 ?
Cl1 Rh1 Rh2 N2 -58(100) . . . 3_655 ?
N1 Rh1 Rh2 N2 21.39(11) . . . . ?
N1 Rh1 Rh2 N2 -68.61(11) 3_655 . . . ?
N1 Rh1 Rh2 N2 -158.61(11) 2_665 . . . ?
N1 Rh1 Rh2 N2 111.39(11) 4_565 . . . ?
Cl1 Rh1 Rh2 N2 -148(100) . . . . ?
N1 Rh1 Rh2 N2 -68.61(11) . . . 4_565 ?
N1 Rh1 Rh2 N2 -158.61(11) 3_655 . . 4_565 ?
N1 Rh1 Rh2 N2 111.39(11) 2_665 . . 4_565 ?
N1 Rh1 Rh2 N2 21.39(11) 4_565 . . 4_565 ?
Cl1 Rh1 Rh2 N2 122(100) . . . 4_565 ?
N1 Rh1 N1 C1 -115.3(3) 3_655 . . . ?
N1 Rh1 N1 C1 158.1(3) 2_665 . . . ?
N1 Rh1 N1 C1 71.5(4) 4_565 . . . ?
Rh2 Rh1 N1 C1 158.1(3) . . . . ?
Cl1 Rh1 N1 C1 -21.9(3) . . . . ?
N1 Rh1 N1 C5 61.7(3) 3_655 . . . ?
N1 Rh1 N1 C5 -24.9(3) 2_665 . . . ?
N1 Rh1 N1 C5 -111.5(2) 4_565 . . . ?
Rh2 Rh1 N1 C5 -24.9(3) . . . . ?
Cl1 Rh1 N1 C5 155.1(3) . . . . ?
N2 Rh2 N2 C5 -25.6(3) 2_665 . . . ?
N2 Rh2 N2 C5 -112.9(3) 3_655 . . . ?
N2 Rh2 N2 C5 61.7(3) 4_565 . . . ?
Rh1 Rh2 N2 C5 -25.6(3) . . . . ?
N2 Rh2 N2 C6 151.6(3) 2_665 . . . ?
N2 Rh2 N2 C6 64.3(3) 3_655 . . . ?
N2 Rh2 N2 C6 -121.1(3) 4_565 . . . ?
Rh1 Rh2 N2 C6 151.6(3) . . . . ?
C5 N1 C1 C2 -3.2(6) . . . . ?
Rh1 N1 C1 C2 173.8(3) . . . . ?
N1 C1 C2 C3 -0.7(7) . . . . ?
C1 C2 C3 C4 1.9(7) . . . . ?
C2 C3 C4 C5 0.7(7) . . . . ?
C6 N2 C5 N1 -164.2(3) . . . . ?
Rh2 N2 C5 N1 13.0(5) . . . . ?
C6 N2 C5 C4 20.2(6) . . . . ?
Rh2 N2 C5 C4 -162.6(3) . . . . ?
C1 N1 C5 N2 -170.2(4) . . . . ?
Rh1 N1 C5 N2 12.7(5) . . . . ?
C1 N1 C5 C4 5.7(5) . . . . ?
Rh1 N1 C5 C4 -171.4(3) . . . . ?
C3 C4 C5 N2 171.0(4) . . . . ?
C3 C4 C5 N1 -4.6(6) . . . . ?
C5 N2 C6 C11 -122.6(4) . . . . ?
Rh2 N2 C6 C11 60.1(4) . . . . ?
C5 N2 C6 C7 63.6(5) . . . . ?
Rh2 N2 C6 C7 -113.7(4) . . . . ?
C11 C6 C7 F1 178.9(4) . . . . ?
N2 C6 C7 F1 -7.1(6) . . . . ?
C11 C6 C7 C8 -0.6(7) . . . . ?
N2 C6 C7 C8 173.4(4) . . . . ?
F1 C7 C8 C9 -179.6(4) . . . . ?
C6 C7 C8 C9 -0.1(7) . . . . ?
C7 C8 C9 C10 0.9(8) . . . . ?
C8 C9 C10 C11 -1.0(7) . . . . ?
C9 C10 C11 C6 0.3(7) . . . . ?
C7 C6 C11 C10 0.5(6) . . . . ?
N2 C6 C11 C10 -173.5(4) . . . . ?
